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Speciation of inorganic selenium using hydride generation method is a widespread analytical method nowadays. However, a reduction step of Se VI to Se IV is necessary as the hydride-forming species is HSeO 3- (oxydation state+IV). This paper describes the development of a batch assisted microwave system allowing a rapid (<5 min) conversion of Se VI...
Poly(ethylene glycol)-modified glucose oxidase was immobilized in a poly(vinyl alcohol) cryogel membrane, obtained by a freezing-thawing cyclic process, to obtain a suitable amperometric glucose sensor. The covalent linkage between PEG and GOD molecule improved the physical immobilization of enzyme in the polymeric matrix, by decreasing its loss in time. Sensor behaviour was evaluated electrochemically...
This work describes a simulation study aimed at establishing the impact of mixture design on the prediction ability of PLS regression models. Data sets are formed by multiplying UV absorbance spectra of 12 PAHs by their concentration profiles. In these case studies, either all possible mixtures of 1-12 components are used or randomly chosen selections of the mixtures. The effects of the number of...
The technique described in this paper represents the modification and combination of two previously existing methods, alkaline fusion and negative thermal ion mass spectrometry (NTIMS). We have used this technique to analyze repeatedly a homogeneous molybdenite powder used as a reference standard in our laboratory. Analyses were made over a period of 18 months, using four different calibrations of...
The resolution of binary mixtures of nalidixic acid (NA) and 7-hydroxymethylnalidixic acid (OH-NA) has been accomplished by partial least squares (PLS) and principal component regression (PCR) multivariate calibration. The method of determination is based on the fluorescence emission of these compounds in the presence of γ-cyclodextrin (γ-CD). The formation of the inclusion compounds gives rise to...
A module for continuous high pressure-temperature leaching is proposed. The overall approach involves the coupling of an extractor with a continuous-flow manifold where the analyte forms a complex with SCN - , which is driven to a flow-cell packed with a suitable material for retention and continuous monitoring of this process which in turn is a way for indirect monitoring of the leaching...
A concise overview (75 references) of the analytical fractionation of aquatic humic substances using sequential-stage ultrafiltration is presented. First, humic substances in aquatic environments and actual problems connected with their fractionation and analysis are briefly considered. The molecular size classification of dissolved humic substances by means of multistage ultrafiltration, with special...
In this paper, cyclic voltammetry, linear sweep voltammetry and chronocoulometry in connection with the hang mercury drop electrode were used to study NiTMpyP and its mixture with DNA. The reduction of NiTMpyP in our experimental conditions involves in 4e reduction of TMpyP. NiTMpyP interacting with DNA forms electrochemically non-active complex DNA-2NiTMpyP, which can not be reduced on the Hg electrode...
Liquid-liquid extraction of Co(II) and Zn(II) by methylisobutylcetone (MIBK) has been studied systematically from NH 4 SCN/H 2 SO 4 media. The influence of sulphuric acid concentration on the percentage of extraction of Co(II) and Zn(II) has been discussed. It is shown that sulphuric acid concentration has not the same effect on distribution curves of Co(II) and Zn(II). Thus,...
The dissociation constants of representative loop (furosemide), thiazide (chlorthiazide and trichlormethiazide) and potassium sparing (amiloride) diuretics in 10, 30, 40, 50 and 70% (w/w) acetonitrile-water mixtures at 298.15 K were determined, in accordance with IUPAC procedures. The variation in pK a values over the whole composition range can be explained by preferential solvation and the...
A method is proposed for the extraction and individual separation of trivalent gallium, indium and thallium from salicylate media using triphenylarsine oxide dissolved in toluene as an extractant. The optimum extraction conditions are evaluated and described. The extracted metal ions are stripped and estimated spectrophotometrically following complexation with 4-(2-pyridylazo) resorcinol. A possible...
A benzoquinone modified basal plane pyrolytic graphite electrode shows electrocatalytic activity for the oxidation of NADH and ascorbic acid in phosphate buffer (pH 7.3). The modified electrode shows a linear variation of catalytic current with concentration in the range 1-10 mM for both NADH and ascorbic acid. The rate constants have been estimated from the surface coverage data.
The ionic product of water, pK w =-log[H + ][OH - ], has been determined in aqueous solutions of sodium perchlorate over the concentration range of 1.0-8.0 M at 25°C from high-precision potentiometric titrations carried out in cells with liquid junction using both glass and hydrogen electrodes. The glass electrode results are systematically lower probably as a result of interference...
The electrochemical copolymerization of 3,4-dihydroxybenzoic acid (3,4-DHBA) and aniline was carried out at microdisk gold electrodes by means of cyclic voltammetric sweep. The polymer obtained on the electrode shows good electrochemical activity and high stability even though in neutral and weakly basic media. It was found that the response current of ascorbic acid was greatly enhanced at this composite...
A new method for the spectrophotometric determination of nickel naphthenate in gasoline in a microemulsion was developed. PAN reacts with nickel(II) forming a red complex with composition 1:2 (metal to ligand) nickel(II)-PAN and absorption maximum at 568 nm. Nickel naphthenate in gasoline can be determined with PAN in a microemulsion, in the pH range 3.0∼10.0 with a molar absorptivity of 4.8 10 ...
For the determination of antimony by hydride generation techniques a pretreatment procedure has been developed for the reduction of Sb(V) to Sb(III) in order to remove the effect of hydrofluoric acid which strongly interferes with the reduction of pentavalent antimony to the trivalent state. It is based on the combined action of l-cysteine and boric acid at 80°C. The pretreatment is effective in both...
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